US5468830A
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Process for preparing organopolysiloxane gum
Assignee: Shin-Etsu Chemical Co Ltd
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Filing: 1994-01-31
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Granted: 1995-11-21
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Expires: 2014-01-31
Abstract
Abstract A siloxane gum is prepared by adding a silane or siloxane having two hydrolyzable groups in a molecule to a silanol-terminated organopolysiloxane in such an amount to give a molar ratio of silanol group/hydrolyzable group of from 0.5 to 3 and effecting condensation polymerization. The resulting organopoly-siloxane has a degree of polymerization of higher than 1,000 and a minimized content of low-molecular weight cyclic siloxanes of less than 5,000 ppm.
Inventors
- 👤 Yoshio Inoue
- 👤 Susumu Sekiguchi
- 👤 Minoru Igarashi
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 00:18
CPC Classifications
C; C08; C08G; C08G77/00; C08G77/04; C08G77/06; C08L; C08L83/00; C08L83/04; C08G77/045; C08G77/14; C08G77/16; C08G77/20; C08G77/22; C08G77/24; C08G77/26; C08G77/70
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
330 words
In a process for preparing an organopolysiloxane gum by effecting condensation polymerization of a silanol-terminated organosiloxane of the following formula (1): ##STR12## wherein R 1 and R 2 each are a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter n is an integer of 2 to 3,000, the improvement comprising adding a silane or siloxane having two hydrolyzable groups in a molecule to said orgnopolysiloxane of formula (1) in such an amount to give a resultant composition having a molar ratio of the silanol groups in said organosiloxane of formula (1) to the hydrolyzable groups in said silane or siloxane of from 0.5 to 3, and condensation polymerizing the resultant composition to form an organopolysiloxane having a high degree of polymerization of at least 1×10 3 and a total content of low-molecular weight cyclic siloxanes having from three to 25 monomer units of up to 5,000 parts by weight per million parts by weight of the organopolysiloxane, wherein the silane or siloxane having two hydrolyzable groups in a molecule is selected from the group consisting of the following formulae (3) to (6): ##STR13## wherein R 3 , R 4 , R 5 , and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group, and letter a is a positive number of 0 to 100; ##STR14## wherein R 3 , R 4 , R 5 and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter c is a positive number of 1 to 100; ##STR15## wherein R 3 , R 4 , R 5 , R 8 and R 9 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group arid letter d is an integer of 2 to 10; and ##STR16## wherein R 3 , R 4 , and R 5 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter e is a positive number of 0 to 1,000.
Claim 2
Dependent Claim
330 words
In a process for preparing an organopolysiloxane gum by effecting condensation polymerization of a silanol-terminated organosiloxane of the following formula (1): ##STR12## wherein R 1 and R 2 each are a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter n is an integer of 2 to 3,000, the improvement comprising adding a silane or siloxane having two hydrolyzable groups in a molecule to said orgnopolysiloxane of formula (1) in such an amount to give a resultant composition having a molar ratio of the silanol groups in said organosiloxane of formula (1) to the hydrolyzable groups in said silane or siloxane of from 0.5 to 3, and condensation polymerizing the resultant composition to form an organopolysiloxane having a high degree of polymerization of at least 1×10 3 and a total content of low-molecular weight cyclic siloxanes having from three to 25 monomer units of up to 5,000 parts by weight per million parts by weight of the organopolysiloxane, wherein the silane or siloxane having two hydrolyzable groups in a molecule is selected from the group consisting of the following formulae (3) to (6): ##STR13## wherein R 3 , R 4 , R 5 , and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group, and letter a is a positive number of 0 to 100; ##STR14## wherein R 3 , R 4 , R 5 and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter c is a positive number of 1 to 100; ##STR15## wherein R 3 , R 4 , R 5 , R 8 and R 9 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group arid letter d is an integer of 2 to 10; and ##STR16## wherein R 3 , R 4 , and R 5 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter e is a positive number of 0 to 1,000.
Claim 3
Dependent Claim
58 words
The process of claim 1, wherein the silane or siloxane having two hydrolyzable groups is selected from the group consisting of the following formulae: ##STR17## wherein R 7 is a methyl, vinyl, trifluoropropyl or phenyl group, Me is methyl, Et is ethyl, Pr is propyl, Bu is butyl, and letter b is an integer of 1 to 100.
Claim 4
Dependent Claim
31 words
The process of claim 1, wherein the resultant composition subject to condensation polymerizing consists essentially of the silanol-terminated organosiloxane and the silane or siloxane having two hydrolyzale groups in a molecule.
Claim 5
Dependent Claim
54 words
The process of claim 1, wherein low-molecular weight siloxanes are fully removed from the silanol-terminated organosiloxane before the condensation polymerization and the organopolysiloxane product has a total content of low-molecular weight cyclic siloxanes having three to 25 monomer units of less than 2,000 parts by weight per million parts by weight of the organopolysiloxane.
Claim 6
Dependent Claim
31 words
The process of claim 1, wherein each of R 1 -R 9 is a hydrocarbon group of 1-10 carbon atoms optionally having hydrogen atoms replaced by halogen atoms or cyano groups.
Claim 7
Dependent Claim
56 words
The process of claim 1, wherein the silane or siloxane having two hydrolyzable groups is of the following formula: ##STR18## wherein R 3 and R 4 are each a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group, R 5 is a methyl, ethyl or butyl group and the letter e is a number 0 to 10.
Claim 8
Dependent Claim
22 words
The process of claim 1, wherein the molar ratio of the silanol groups to the hydrolyzable groups is from 0.8 to 1.5.
Claim 9
Dependent Claim
17 words
The process of claim 1, wherein the condensation polymerization temperature is from room temperature to 200° C.
Claim 10
Dependent Claim
19 words
The process of claim 1, wherein the organopolysiloxane has a degree of polymerization of at least 5×10 3 .
Claim 11
Dependent Claim
190 words
In a process for preparing an organopolysiloxane gum by effecting condensation polymerization of a silanol-terminated organosiloxane of the following formula (1): ##STR19## wherein R 1 and R 2 each are a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter n is an integer of 2 to 3,000, the improvement which comprises adding a silane or siloxane having two hydrolyzable groups in a molecule to said organopolysiloxane of formula (1) in such an amount to give a resultant composition having a molar ratio of the silanol groups in said organosiloxane having a high degree of polymerization of formula (1) to the hydrolyzable groups in said silane or siloxane of from 0.5 to 3, and condensation polymerizing the resultant composition to form an organopolysiloxane having a high degree of polymerization of at least 1×10 3 and a total content of low-molecular weight cyclic siloxanes having from three to 25 monomer units of up to 5,000 parts by weight per million parts by weight of the organopolysiloxane, wherein the resultant composition subject to the condensation polymerization consists essentially of the silanol-terminated organosiloxane and the silane or siloxane having two hydrolyzable groups.
Claim 12
Dependent Claim
190 words
In a process for preparing an organopolysiloxane gum by effecting condensation polymerization of a silanol-terminated organosiloxane of the following formula (1): ##STR19## wherein R 1 and R 2 each are a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter n is an integer of 2 to 3,000, the improvement which comprises adding a silane or siloxane having two hydrolyzable groups in a molecule to said organopolysiloxane of formula (1) in such an amount to give a resultant composition having a molar ratio of the silanol groups in said organosiloxane having a high degree of polymerization of formula (1) to the hydrolyzable groups in said silane or siloxane of from 0.5 to 3, and condensation polymerizing the resultant composition to form an organopolysiloxane having a high degree of polymerization of at least 1×10 3 and a total content of low-molecular weight cyclic siloxanes having from three to 25 monomer units of up to 5,000 parts by weight per million parts by weight of the organopolysiloxane, wherein the resultant composition subject to the condensation polymerization consists essentially of the silanol-terminated organosiloxane and the silane or siloxane having two hydrolyzable groups.
Claim 13
Dependent Claim
175 words
The process of claim 10, wherein the silane or siloxane having two hydrolyzable groups in a molecule is selected from the group consisting of the following formulae (3) to (6): ##STR20## wherein R 3 , R 4 , R 5 , and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group, and letter a is a positive number of 0 to 100; ##STR21## wherein R 3 , R 4 , R 5 and R 6 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter c is a positive number of 1 to 100; ##STR22## wherein R 3 , R 4 , R 5 , R 8 and R 9 are each independently a halogen-or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter d is an integer of 2 to 10; and ##STR23## wherein R 3 , R 4 , and R 5 are each independently a halogen- or cyano-substituted or unsubstituted monovalent hydrocarbon group and letter e is a positive number of 0 to 1,000.
Claim 14
Dependent Claim
58 words
The process of claim 10, wherein the silane or siloxane having two hydrolyzable groups is selected from the group consisting of the following formulae: ##STR24## wherein R 7 is a methyl, vinyl, trifluoropropyl or phenyl group, Me is methyl, Et is ethyl, Pr is propyl, Bu is butyl, and letter b is an integer of 1 to 100.
Claim 15
Dependent Claim
54 words
The process of claim 10, wherein low-molecular weight siloxanes are fully removed from the silanol-terminated organosiloxane before the condensation polymerization and the organopolysiloxane product has a total content of low-molecular weight cyclic siloxanes having three to 25 monomer units of less than 2,000 parts by weight per million parts by weight of the organopolysiloxane.
Claim 16
Dependent Claim
28 words
The process of claim 11, wherein each of R 1 -R 9 is a hydrocarbon group of 1-10 carbon atoms optionally substituted by halogen atoms or cyano groups.
Claim 17
Dependent Claim
56 words
The process of claim 1, wherein the silane or siloxane having two hydrolyzable groups is of the following formula: ##STR25## wherein R 3 and R 4 are each a halogen- or cyan-substituted or unsubstituted monovalent hydrocarbon group, R 5 is a methyl, ethyl or butyl group and the letter e is a number 0 to 10.
Claim 18
Dependent Claim
22 words
The process of claim 10, wherein the molar ratio of the silanol groups to the hydrolyzable groups is from 0.8 to 1.5.
Claim 19
Dependent Claim
17 words
The process of claim 10, wherein the condensation polymerization temperature is from room temperature to 200° C.
Claim 20
Dependent Claim
19 words
The process of claim 10, wherein the organopolysiloxane has a degree of polymerization of at least 5×10 3 .
References Cited (Backward Citations)
US4673750A
Cited
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